毛细管气相色谱法测定间尼索地平原料药中有机溶剂残留量___

摘要　目的：建立间尼索地平原料药中3种有机溶剂残留量的气相色谱测定方法。方法：采用毛细管气相色谱法，以二甲基甲酰胺为溶剂，HP-INNOWax毛细管柱（30m×0.53mm×3.0μm），FID检测器。结果：3种有机溶剂丙酮、甲醇、乙醇均达到了完全分离，在考察的浓度范围内具有良好线性，丙酮、甲醇、乙醇的最低检测浓度分别为0.08，0.06，0.08 μg•mL-1，精密度RSD均小于2.0%，平均回收率为95%~105%。样品均符合要求。结论：该方法灵敏度、准确度均达到有机溶剂残留量的检测要求，可用于间尼索地平原料药中3种残留溶剂的同时检测与分析。

 

Abstract Objective: To develop a capillary GC method for simultaneous determining the residual organic solvents acetone, methanol and ethanol in m-nisoldipine. Methods: The samples were dissolved in N,N-dimethylformamide. The three organic solvents were separated on a HP-INNOWax capillary column（30m×0.53mm×3.0μm）using programmable increased temperature. The intial temperature was kept at 50℃ for 2 min and then up to 80℃ at the rate of 5℃•min-1 for 1 min and eventually raised to 180℃ at the rate of 40℃•min-1 for 5 min. Results: Three residual organic solvents consisting of acetone, methanol and ethanol in m-nisoldipine were completely separated. It appears a good linearity in the experimental concentration. The limit of detection for acetone, methanol and ethanol were 0.08, 0.06 and 0.08 μg•mL-1, respectively. The RSD values of precision were all less than 2.0%. The average recoveries were 95%~105% and the samples coincided with the requirements. Conclusion: The method was proved to be accurate and sensitive after validation. It is suitable to determine residual organic solvents in m-nisoldipine.